Preparation of rifampin
A technology of rifampicin and rifamycin, applied in organic chemistry, antibacterial drugs, etc., can solve problems such as high cost and unsatisfactory product quality
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[0029] The operation steps of the first batch and subsequent batch preparation methods of high-quality rifampicin of the present invention are as follows:
[0030] Step one salt reaction
[0031] In the first batch of production, the rifamycin SV is oxidized to produce S and then extracted with BA to obtain the S-BA feed liquid as the starting material, concentrated to 100-140 thousand u / ml, from which 50 million units are taken S-BA concentrated feed solution of S, drop 100-250ml of 6% sodium bicarbonate aqueous solution, control 30~50℃ to react for 3~6h to generate S sodium salt, cool to no higher than 10℃, crystallize and filter to obtain the product, and recover the mother liquor To be recycled. When continuing batch production, you can also directly take the S-BA concentrated feed solution equivalent to 50 million units of rifamycin S and the previous batch of recovered mother liquor, repeat the above-mentioned salt formation reaction, and regularly neutralize the recovered m...
Embodiment 1
[0039] The rifamycin SV is oxidized to produce S, and then extracted with BA to obtain the S-BA feed liquid as the starting material, which is concentrated to 100,000 to 140,000 u / ml, and 50 million units of S are taken from the concentrated feed liquid Add 150ml of 6% sodium bicarbonate aqueous solution at 45℃ and maintain the reaction for 5h. After the reaction, the temperature will be cooled to 10℃ and the crystal will be filtered by suction. The filter cake will be washed with purified water and then drained. Controlled at 60℃ and dried under reduced pressure to obtain S The sodium salt is about 45 grams, and the mother liquor is recovered for recycling. Sodium salt was added to 90ml DMF containing 3.8ml of acetic acid, stirred at 50°C for 30 minutes to be freed into S, and then 14.4ml of dihydroxy cyclization reaction was added dropwise for 1 hour to obtain oxazine. DMF is recovered by molecular distillation. After recovery, an appropriate amount of ethanol is added to dis...
Embodiment 2
[0041] The rifamycin SV is oxidized to produce S and then extracted with BA to obtain the S-BA feed liquid as the starting material, and then concentrate to 100-140 thousand u / ml, and take 50 million units of S from the concentrated feed liquid Add 150ml of 6% sodium bicarbonate aqueous solution at 45℃ and maintain the reaction for 5h. After the reaction, the temperature will be cooled to 10℃ and the crystallization will be filtered by suction. The filter cake will be washed with purified water and drained. Controlled at 60℃ and dried under reduced pressure to obtain S The sodium salt is about 45 grams, and the mother liquor is recovered for recycling. Sodium salt was added to 90ml DMF containing 3.8ml of acetic acid, stirred at 50°C for 30 minutes to be freed into S, and then 14.4ml of dihydroxy cyclization reaction was added dropwise for 1 hour to obtain oxazine. DMF is recovered by molecular distillation. After recovery, an appropriate amount of ethanol is added to dissolve ...
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